# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'ProfD Chen-Wei Liu' _publ_contact_author_address ; ? ; _publ_contact_author_email CHENWEI@CYCU.EDU.TW _publ_section_title ; A 2D honeycomb-shaped network based on a starburst cluster:[Ag4(Cl)(PPh2(CH2)2PPh2)1.5{S2P(OR)2}3](R = Et, iPr) ; loop_ _publ_author_name 'Chen-Wei Liu' 'Ben-Jie Liaw' 'Lin-Shou Liou' 'Ju-Chun Wang' data_1a _database_code_depnum_ccdc_archive 'CCDC 254826' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H34 Ag O2 P3 S2' _chemical_formula_weight 691.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.954(2) _cell_length_b 12.985(2) _cell_length_c 13.116(2) _cell_angle_alpha 61.926(3) _cell_angle_beta 77.409(3) _cell_angle_gamma 68.296(3) _cell_volume 1666.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 936 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 24.98 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 0.898 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7294 _exptl_absorpt_correction_T_max 0.9561 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7845 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0181 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5606 _reflns_number_gt 5055 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+2.7828P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5606 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1177 _refine_ls_wR_factor_gt 0.1070 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.81407(3) 0.80532(3) 0.59629(3) 0.05845(13) Uani 1 1 d . . . S1 S 0.77162(19) 0.61799(13) 0.78400(13) 0.0973(5) Uani 1 1 d . . . S2 S 0.73357(15) 0.89759(12) 0.75631(12) 0.0817(4) Uani 1 1 d . . . P1 P 0.74132(13) 0.72501(13) 0.86011(11) 0.0734(3) Uani 1 1 d . . . P2 P 0.67483(9) 0.89604(9) 0.44010(9) 0.0463(2) Uani 1 1 d . . . P3 P 1.02092(9) 0.81395(9) 0.52044(9) 0.0484(2) Uani 1 1 d . . . O1 O 0.6344(5) 0.7110(5) 0.9537(4) 0.1271(17) Uani 1 1 d . . . O2 O 0.8456(5) 0.6606(4) 0.9487(5) 0.1272(18) Uani 1 1 d . . . C1 C 0.5177(9) 0.7570(13) 0.9179(9) 0.223(7) Uani 1 1 d . . . H1A H 0.5176 0.7401 0.8534 0.268 Uiso 1 1 calc R . . H1B H 0.4888 0.8453 0.8918 0.268 Uiso 1 1 calc R . . C2 C 0.4401(12) 0.703(2) 1.0087(13) 0.416(19) Uani 1 1 d . . . H2A H 0.3601 0.7364 0.9822 0.624 Uiso 1 1 calc R . . H2B H 0.4392 0.7213 1.0722 0.624 Uiso 1 1 calc R . . H2C H 0.4680 0.6162 1.0339 0.624 Uiso 1 1 calc R . . C3 C 0.8605(15) 0.7145(11) 1.0119(12) 0.241(8) Uani 1 1 d . . . H3A H 0.8849 0.7856 0.9565 0.290 Uiso 1 1 calc R . . H3B H 0.7810 0.7457 1.0434 0.290 Uiso 1 1 calc R . . C4 C 0.9283(15) 0.6607(10) 1.0914(12) 0.253(9) Uani 1 1 d . . . H4A H 0.9189 0.7136 1.1269 0.379 Uiso 1 1 calc R . . H4B H 1.0101 0.6384 1.0620 0.379 Uiso 1 1 calc R . . H4C H 0.9089 0.5880 1.1478 0.379 Uiso 1 1 calc R . . C11 C 0.6225(3) 0.7906(4) 0.4221(4) 0.0536(9) Uani 1 1 d . . . C12 C 0.6802(5) 0.6659(4) 0.4783(5) 0.0799(15) Uani 1 1 d . . . H12A H 0.7390 0.6371 0.5298 0.096 Uiso 1 1 calc R . . C13 C 0.6505(6) 0.5834(6) 0.4581(8) 0.111(2) Uani 1 1 d . . . H13A H 0.6905 0.4998 0.4949 0.133 Uiso 1 1 calc R . . C14 C 0.5634(7) 0.6246(6) 0.3850(7) 0.109(2) Uani 1 1 d . . . H14A H 0.5444 0.5692 0.3712 0.130 Uiso 1 1 calc R . . C15 C 0.5029(5) 0.7479(6) 0.3309(6) 0.0947(18) Uani 1 1 d . . . H15A H 0.4417 0.7753 0.2824 0.114 Uiso 1 1 calc R . . C16 C 0.5329(4) 0.8317(5) 0.3485(5) 0.0710(12) Uani 1 1 d . . . H16A H 0.4927 0.9153 0.3109 0.085 Uiso 1 1 calc R . . C21 C 0.7471(3) 0.9675(4) 0.2982(3) 0.0514(9) Uani 1 1 d . . . C22 C 0.7829(5) 0.9175(5) 0.2205(5) 0.0894(18) Uani 1 1 d . . . H22A H 0.7662 0.8464 0.2376 0.107 Uiso 1 1 calc R . . C23 C 0.8440(6) 0.9715(7) 0.1163(6) 0.106(2) Uani 1 1 d . . . H23A H 0.8645 0.9382 0.0631 0.128 Uiso 1 1 calc R . . C24 C 0.8740(5) 1.0716(6) 0.0916(5) 0.0874(16) Uani 1 1 d . . . H24A H 0.9167 1.1062 0.0227 0.105 Uiso 1 1 calc R . . C25 C 0.8415(6) 1.1207(6) 0.1675(5) 0.0931(18) Uani 1 1 d . . . H25A H 0.8615 1.1899 0.1508 0.112 Uiso 1 1 calc R . . C26 C 0.7783(5) 1.0696(5) 0.2707(4) 0.0797(15) Uani 1 1 d . . . H26A H 0.7567 1.1050 0.3223 0.096 Uiso 1 1 calc R . . C31 C 1.0783(4) 0.7665(4) 0.4029(3) 0.0516(9) Uani 1 1 d . . . C32 C 1.0517(4) 0.6670(4) 0.4120(4) 0.0657(11) Uani 1 1 d . . . H32A H 1.0040 0.6295 0.4749 0.079 Uiso 1 1 calc R . . C33 C 1.0953(5) 0.6231(5) 0.3287(5) 0.0801(14) Uani 1 1 d . . . H33A H 1.0776 0.5558 0.3362 0.096 Uiso 1 1 calc R . . C34 C 1.1640(5) 0.6779(5) 0.2359(5) 0.0820(15) Uani 1 1 d . . . H34A H 1.1946 0.6473 0.1806 0.098 Uiso 1 1 calc R . . C35 C 1.1884(5) 0.7791(6) 0.2237(5) 0.0865(16) Uani 1 1 d . . . H35A H 1.2338 0.8179 0.1593 0.104 Uiso 1 1 calc R . . C36 C 1.1455(5) 0.8229(5) 0.3073(4) 0.0728(13) Uani 1 1 d . . . H36A H 1.1623 0.8912 0.2987 0.087 Uiso 1 1 calc R . . C41 C 1.1464(4) 0.7287(3) 0.6161(4) 0.0540(9) Uani 1 1 d . . . C42 C 1.2633(4) 0.7306(4) 0.5756(5) 0.0694(12) Uani 1 1 d . . . H42A H 1.2787 0.7758 0.4972 0.083 Uiso 1 1 calc R . . C43 C 1.3571(5) 0.6669(5) 0.6488(6) 0.0875(17) Uani 1 1 d . . . H43A H 1.4348 0.6700 0.6209 0.105 Uiso 1 1 calc R . . C44 C 1.3330(7) 0.5982(6) 0.7649(7) 0.105(2) Uani 1 1 d . . . H44A H 1.3956 0.5535 0.8152 0.126 Uiso 1 1 calc R . . C45 C 1.2194(7) 0.5954(6) 0.8059(6) 0.103(2) Uani 1 1 d . . . H45A H 1.2048 0.5496 0.8844 0.124 Uiso 1 1 calc R . . C46 C 1.1242(5) 0.6600(5) 0.7326(5) 0.0777(13) Uani 1 1 d . . . H46A H 1.0466 0.6570 0.7614 0.093 Uiso 1 1 calc R . . C51 C 0.5380(3) 1.0216(3) 0.4442(3) 0.0495(9) Uani 1 1 d . . . H51A H 0.5611 1.0888 0.4375 0.059 Uiso 1 1 calc R . . H51B H 0.4905 1.0518 0.3789 0.059 Uiso 1 1 calc R . . C61 C 1.0263(4) 0.9720(3) 0.4570(3) 0.0509(9) Uani 1 1 d . . . H61A H 1.1093 0.9721 0.4353 0.061 Uiso 1 1 calc R . . H61B H 0.9810 1.0213 0.3877 0.061 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0591(2) 0.0600(2) 0.0566(2) -0.02341(15) 0.00025(14) -0.02285(15) S1 0.1547(15) 0.0673(8) 0.0731(9) -0.0260(7) 0.0145(9) -0.0551(9) S2 0.1113(11) 0.0634(7) 0.0697(8) -0.0340(6) 0.0041(7) -0.0242(7) P1 0.0850(9) 0.0810(9) 0.0573(7) -0.0281(6) 0.0065(6) -0.0370(7) P2 0.0425(5) 0.0451(5) 0.0538(5) -0.0257(4) 0.0014(4) -0.0125(4) P3 0.0494(5) 0.0441(5) 0.0542(6) -0.0222(4) -0.0006(4) -0.0171(4) O1 0.124(4) 0.145(4) 0.084(3) -0.038(3) 0.023(3) -0.044(3) O2 0.171(5) 0.099(3) 0.113(4) -0.025(3) -0.055(3) -0.043(3) C1 0.106(7) 0.273(15) 0.132(8) -0.013(9) -0.016(6) 0.014(8) C2 0.118(9) 0.55(4) 0.173(13) 0.050(17) 0.044(9) 0.013(14) C3 0.36(2) 0.179(11) 0.232(14) -0.060(10) -0.191(15) -0.069(12) C4 0.42(2) 0.125(8) 0.252(15) -0.050(9) -0.217(16) -0.050(11) C11 0.047(2) 0.054(2) 0.067(2) -0.034(2) 0.0047(18) -0.0171(17) C12 0.071(3) 0.049(2) 0.121(5) -0.038(3) -0.018(3) -0.012(2) C13 0.104(5) 0.067(3) 0.181(7) -0.067(4) -0.016(5) -0.024(3) C14 0.107(5) 0.096(5) 0.171(7) -0.089(5) 0.001(5) -0.045(4) C15 0.082(4) 0.119(5) 0.123(5) -0.075(4) -0.011(3) -0.039(4) C16 0.068(3) 0.068(3) 0.089(3) -0.043(3) -0.010(2) -0.019(2) C21 0.049(2) 0.055(2) 0.052(2) -0.0263(18) 0.0007(17) -0.0154(17) C22 0.103(4) 0.092(4) 0.098(4) -0.066(3) 0.046(3) -0.052(3) C23 0.128(5) 0.130(5) 0.096(4) -0.082(4) 0.054(4) -0.066(5) C24 0.088(4) 0.106(4) 0.070(3) -0.038(3) 0.022(3) -0.045(3) C25 0.119(5) 0.088(4) 0.084(4) -0.039(3) 0.029(3) -0.061(4) C26 0.105(4) 0.084(3) 0.070(3) -0.042(3) 0.023(3) -0.052(3) C31 0.050(2) 0.052(2) 0.056(2) -0.0251(18) -0.0028(17) -0.0163(17) C32 0.080(3) 0.053(2) 0.070(3) -0.030(2) 0.000(2) -0.025(2) C33 0.103(4) 0.067(3) 0.086(4) -0.042(3) -0.013(3) -0.026(3) C34 0.094(4) 0.089(4) 0.077(3) -0.053(3) -0.002(3) -0.022(3) C35 0.093(4) 0.117(5) 0.071(3) -0.052(3) 0.016(3) -0.051(4) C36 0.083(3) 0.088(3) 0.071(3) -0.045(3) 0.014(2) -0.048(3) C41 0.057(2) 0.043(2) 0.065(2) -0.0257(19) -0.0096(18) -0.0121(17) C42 0.060(3) 0.066(3) 0.088(3) -0.041(3) -0.013(2) -0.009(2) C43 0.065(3) 0.082(4) 0.131(5) -0.063(4) -0.028(3) -0.003(3) C44 0.104(5) 0.078(4) 0.130(6) -0.045(4) -0.062(5) 0.006(4) C45 0.128(6) 0.079(4) 0.079(4) -0.011(3) -0.039(4) -0.021(4) C46 0.085(3) 0.063(3) 0.072(3) -0.017(2) -0.016(3) -0.019(3) C51 0.048(2) 0.0416(19) 0.057(2) -0.0252(17) 0.0029(17) -0.0098(16) C61 0.052(2) 0.0434(19) 0.057(2) -0.0215(17) 0.0016(17) -0.0163(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P2 2.4737(11) . ? Ag1 P3 2.4786(11) . ? Ag1 S1 2.6396(14) . ? Ag1 S2 2.7204(14) . ? S1 P1 1.958(2) . ? S2 P1 1.978(2) . ? P1 O1 1.565(5) . ? P1 O2 1.597(5) . ? P2 C11 1.824(4) . ? P2 C21 1.828(4) . ? P2 C51 1.846(4) . ? P3 C41 1.826(4) . ? P3 C31 1.829(4) . ? P3 C61 1.838(4) . ? O1 C1 1.389(11) . ? O2 C3 1.381(11) . ? C1 C2 1.406(16) . ? C3 C4 1.224(12) . ? C11 C16 1.381(6) . ? C11 C12 1.383(6) . ? C12 C13 1.390(8) . ? C13 C14 1.352(10) . ? C14 C15 1.374(9) . ? C15 C16 1.388(7) . ? C21 C22 1.366(6) . ? C21 C26 1.372(6) . ? C22 C23 1.391(8) . ? C23 C24 1.350(8) . ? C24 C25 1.339(8) . ? C25 C26 1.386(7) . ? C31 C36 1.374(6) . ? C31 C32 1.388(6) . ? C32 C33 1.382(7) . ? C33 C34 1.358(8) . ? C34 C35 1.379(8) . ? C35 C36 1.384(7) . ? C41 C46 1.383(7) . ? C41 C42 1.388(6) . ? C42 C43 1.378(7) . ? C43 C44 1.384(10) . ? C44 C45 1.355(10) . ? C45 C46 1.391(8) . ? C51 C51 1.518(7) 2_676 ? C61 C61 1.523(8) 2_776 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Ag1 P3 112.44(4) . . ? P2 Ag1 S1 114.86(5) . . ? P3 Ag1 S1 122.51(5) . . ? P2 Ag1 S2 114.27(4) . . ? P3 Ag1 S2 110.73(4) . . ? S1 Ag1 S2 76.97(5) . . ? P1 S1 Ag1 84.32(6) . . ? P1 S2 Ag1 81.80(6) . . ? O1 P1 O2 96.3(3) . . ? O1 P1 S1 111.9(2) . . ? O2 P1 S1 105.7(2) . . ? O1 P1 S2 113.7(2) . . ? O2 P1 S2 111.2(2) . . ? S1 P1 S2 115.87(9) . . ? C11 P2 C21 102.46(19) . . ? C11 P2 C51 105.67(18) . . ? C21 P2 C51 103.24(18) . . ? C11 P2 Ag1 116.82(14) . . ? C21 P2 Ag1 111.22(13) . . ? C51 P2 Ag1 115.78(14) . . ? C41 P3 C31 102.53(19) . . ? C41 P3 C61 102.30(19) . . ? C31 P3 C61 104.25(18) . . ? C41 P3 Ag1 120.85(15) . . ? C31 P3 Ag1 114.10(13) . . ? C61 P3 Ag1 110.97(13) . . ? C1 O1 P1 119.0(6) . . ? C3 O2 P1 122.8(7) . . ? O1 C1 C2 110.9(10) . . ? C4 C3 O2 123.9(12) . . ? C16 C11 C12 119.3(4) . . ? C16 C11 P2 122.0(3) . . ? C12 C11 P2 118.6(3) . . ? C11 C12 C13 120.1(6) . . ? C14 C13 C12 120.2(6) . . ? C13 C14 C15 120.4(5) . . ? C14 C15 C16 120.2(6) . . ? C11 C16 C15 119.7(5) . . ? C22 C21 C26 117.1(4) . . ? C22 C21 P2 123.0(4) . . ? C26 C21 P2 119.5(3) . . ? C21 C22 C23 121.0(5) . . ? C24 C23 C22 120.6(5) . . ? C25 C24 C23 119.2(5) . . ? C24 C25 C26 120.9(5) . . ? C21 C26 C25 121.1(5) . . ? C36 C31 C32 118.5(4) . . ? C36 C31 P3 124.1(3) . . ? C32 C31 P3 117.4(3) . . ? C33 C32 C31 120.7(5) . . ? C34 C33 C32 120.2(5) . . ? C33 C34 C35 119.9(5) . . ? C34 C35 C36 120.1(5) . . ? C31 C36 C35 120.5(5) . . ? C46 C41 C42 119.0(4) . . ? C46 C41 P3 119.0(4) . . ? C42 C41 P3 122.0(4) . . ? C43 C42 C41 121.5(5) . . ? C42 C43 C44 118.6(6) . . ? C45 C44 C43 120.7(6) . . ? C44 C45 C46 121.0(6) . . ? C41 C46 C45 119.2(6) . . ? C51 C51 P2 111.3(3) 2_676 . ? C61 C61 P3 110.7(3) 2_776 . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 1.090 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.076 #===END data_2a _database_code_depnum_ccdc_archive 'CCDC 254827' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H66 Ag4 Cl O6 P6 S6' _chemical_formula_weight 1620.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 19.7782(16) _cell_length_b 19.7782(16) _cell_length_c 32.244(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10923.2(18) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 33 _cell_measurement_theta_min 5.23 _cell_measurement_theta_max 12.26 _exptl_crystal_description block _exptl_crystal_colour coloress _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4866 _exptl_absorpt_coefficient_mu 1.439 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.720 _exptl_absorpt_correction_T_max 0.890 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 497 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3830 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 22.50 _reflns_number_total 3123 _reflns_number_gt 2099 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0895P)^2^+62.0762P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3123 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0947 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1824 _refine_ls_wR_factor_gt 0.1591 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.6667 0.3333 1.08051(4) 0.0879(5) Uani 1 3 d S . . Ag2 Ag 0.61437(6) 0.20044(5) 1.01030(3) 0.1045(4) Uani 1 1 d . . . Cl1 Cl 0.6667 0.3333 0.97126(14) 0.0801(11) Uani 1 3 d S . . S1 S 0.54562(17) 0.34254(17) 1.08669(9) 0.0918(8) Uani 1 1 d . . . S2 S 0.46973(17) 0.18507(17) 1.02309(11) 0.1052(10) Uani 1 1 d . . . P1 P 0.46233(17) 0.23183(19) 1.07455(10) 0.0982(9) Uani 1 1 d . . . P2 P 0.59223(15) 0.09550(13) 0.96262(7) 0.0706(7) Uani 1 1 d . . . O1 O 0.3801(5) 0.2218(7) 1.0801(3) 0.151(4) Uani 1 1 d . . . O2 O 0.4588(6) 0.1741(7) 1.1102(4) 0.175(5) Uani 1 1 d . . . C1 C 0.3486(16) 0.2484(15) 1.0500(6) 0.225(12) Uani 1 1 d . . . H1A H 0.3792 0.3049 1.0513 0.269 Uiso 1 1 calc R . . H1B H 0.3614 0.2337 1.0237 0.269 Uiso 1 1 calc R . . C2 C 0.2759(11) 0.232(2) 1.0464(8) 0.32(2) Uani 1 1 d . . . H2A H 0.2711 0.2588 1.0228 0.483 Uiso 1 1 calc R . . H2B H 0.2607 0.2485 1.0710 0.483 Uiso 1 1 calc R . . H2C H 0.2427 0.1767 1.0428 0.483 Uiso 1 1 calc R . . C3 C 0.4588(15) 0.1819(15) 1.1494(6) 0.225(11) Uani 1 1 d . . . H3A H 0.4133 0.1857 1.1569 0.271 Uiso 1 1 calc R . . H3B H 0.5046 0.2307 1.1570 0.271 Uiso 1 1 calc R . . C4 C 0.458(2) 0.122(2) 1.1724(7) 0.37(2) Uani 1 1 d . . . H4A H 0.4583 0.1326 1.2015 0.553 Uiso 1 1 calc R . . H4B H 0.5036 0.1184 1.1658 0.553 Uiso 1 1 calc R . . H4C H 0.4121 0.0733 1.1658 0.553 Uiso 1 1 calc R . . C5 C 0.5343(6) 0.0017(5) 0.9893(3) 0.078(3) Uani 1 1 d . . . H5A H 0.5163 -0.0405 0.9694 0.117 Uiso 1 1 calc R . . H5B H 0.5667 -0.0051 1.0095 0.117 Uiso 1 1 calc R . . C11 C 0.6745(6) 0.0899(6) 0.9416(3) 0.081(3) Uani 1 1 d . . . C12 C 0.6713(8) 0.0200(8) 0.9329(4) 0.116(4) Uani 1 1 d . . . H12A H 0.6253 -0.0271 0.9368 0.139 Uiso 1 1 calc R . . C13 C 0.7376(10) 0.0210(10) 0.9181(5) 0.141(5) Uani 1 1 d . . . H13A H 0.7361 -0.0257 0.9120 0.169 Uiso 1 1 calc R . . C14 C 0.8061(9) 0.0913(13) 0.9125(5) 0.145(6) Uani 1 1 d . . . H14A H 0.8515 0.0915 0.9045 0.174 Uiso 1 1 calc R . . C15 C 0.8072(9) 0.1582(11) 0.9185(5) 0.139(5) Uani 1 1 d . . . H15A H 0.8520 0.2052 0.9123 0.166 Uiso 1 1 calc R . . C16 C 0.7423(7) 0.1586(7) 0.9338(4) 0.103(3) Uani 1 1 d . . . H16A H 0.7444 0.2059 0.9390 0.124 Uiso 1 1 calc R . . C21 C 0.5347(5) 0.0888(6) 0.9175(3) 0.073(2) Uani 1 1 d . . . C22 C 0.4865(7) 0.0214(7) 0.8979(3) 0.113(4) Uani 1 1 d . . . H22A H 0.4812 -0.0253 0.9076 0.136 Uiso 1 1 calc R . . C23 C 0.4448(9) 0.0211(11) 0.8637(4) 0.152(6) Uani 1 1 d . . . H23A H 0.4105 -0.0263 0.8512 0.183 Uiso 1 1 calc R . . C24 C 0.4523(9) 0.0877(12) 0.8475(4) 0.129(5) Uani 1 1 d . . . H24A H 0.4254 0.0865 0.8236 0.155 Uiso 1 1 calc R . . C25 C 0.4998(9) 0.1558(10) 0.8668(4) 0.123(4) Uani 1 1 d . . . H25A H 0.5052 0.2022 0.8566 0.147 Uiso 1 1 calc R . . C26 C 0.5402(7) 0.1567(7) 0.9017(3) 0.096(3) Uani 1 1 d . . . H26A H 0.5720 0.2039 0.9150 0.115 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0856(6) 0.0856(6) 0.0926(10) 0.000 0.000 0.0428(3) Ag2 0.1331(8) 0.0732(6) 0.0995(7) -0.0134(4) -0.0251(5) 0.0458(5) Cl1 0.0665(15) 0.0665(15) 0.107(3) 0.000 0.000 0.0333(7) S1 0.098(2) 0.0951(19) 0.0933(18) 0.0024(15) 0.0135(15) 0.0571(17) S2 0.0860(19) 0.0809(18) 0.148(3) -0.0027(18) 0.0048(18) 0.0409(15) P1 0.0780(18) 0.108(2) 0.100(2) 0.0289(18) 0.0183(15) 0.0406(17) P2 0.0776(16) 0.0601(14) 0.0657(14) 0.0092(11) 0.0070(12) 0.0281(12) O1 0.108(7) 0.185(10) 0.154(9) 0.003(7) 0.031(6) 0.069(7) O2 0.156(9) 0.165(9) 0.139(9) 0.062(8) 0.006(7) 0.032(7) C1 0.31(3) 0.33(3) 0.181(18) 0.117(19) 0.11(2) 0.27(3) C2 0.119(15) 0.59(6) 0.25(3) 0.16(3) 0.052(16) 0.18(3) C3 0.26(3) 0.28(3) 0.131(15) 0.089(17) 0.044(16) 0.13(2) C4 0.66(7) 0.43(5) 0.134(18) 0.10(3) 0.05(3) 0.36(5) C5 0.098(7) 0.067(6) 0.070(6) 0.013(5) 0.021(5) 0.042(5) C11 0.077(7) 0.081(7) 0.075(6) 0.021(5) 0.009(5) 0.031(6) C12 0.110(9) 0.099(9) 0.134(10) 0.029(8) 0.043(8) 0.050(8) C13 0.148(13) 0.168(14) 0.155(13) 0.049(11) 0.060(11) 0.116(13) C14 0.095(11) 0.202(18) 0.148(13) 0.058(13) 0.040(9) 0.082(13) C15 0.103(11) 0.159(15) 0.136(12) 0.032(11) 0.022(9) 0.053(11) C16 0.088(8) 0.105(9) 0.102(8) 0.016(7) 0.000(7) 0.037(7) C21 0.071(6) 0.073(6) 0.067(6) 0.003(5) 0.008(5) 0.029(5) C22 0.121(9) 0.100(9) 0.076(7) 0.004(6) -0.020(7) 0.023(7) C23 0.129(12) 0.172(16) 0.092(10) -0.001(10) -0.023(9) 0.028(11) C24 0.139(12) 0.205(18) 0.060(8) 0.009(10) -0.013(8) 0.098(13) C25 0.170(14) 0.159(13) 0.080(9) 0.004(9) -0.011(9) 0.112(12) C26 0.114(9) 0.094(8) 0.087(8) -0.004(6) -0.006(6) 0.057(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 S1 2.498(3) 2_655 ? Ag1 S1 2.498(3) 3_665 ? Ag1 S1 2.498(3) . ? Ag1 Ag2 3.2225(13) . ? Ag1 Ag2 3.2225(13) 2_655 ? Ag1 Ag2 3.2225(13) 3_665 ? Ag2 P2 2.440(3) . ? Ag2 S1 2.598(3) 2_655 ? Ag2 Cl1 2.616(2) . ? Ag2 S2 2.753(3) . ? Cl1 Ag2 2.616(2) 2_655 ? Cl1 Ag2 2.616(2) 3_665 ? S1 P1 2.013(4) . ? S1 Ag2 2.598(3) 3_665 ? S2 P1 1.941(5) . ? P1 O1 1.547(10) . ? P1 O2 1.597(11) . ? P2 C21 1.810(10) . ? P2 C11 1.817(11) . ? P2 C5 1.836(9) . ? O1 C1 1.389(19) . ? O2 C3 1.27(2) . ? C1 C2 1.31(2) . ? C3 C4 1.40(3) . ? C5 C5 1.493(17) 10_657 ? C11 C16 1.371(14) . ? C11 C12 1.382(15) . ? C12 C13 1.386(17) . ? C13 C14 1.38(2) . ? C14 C15 1.33(2) . ? C15 C16 1.380(18) . ? C21 C22 1.348(14) . ? C21 C26 1.389(14) . ? C22 C23 1.376(18) . ? C23 C24 1.35(2) . ? C24 C25 1.350(19) . ? C25 C26 1.373(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ag1 S1 119.37(2) 2_655 3_665 ? S1 Ag1 S1 119.37(2) 2_655 . ? S1 Ag1 S1 119.37(2) 3_665 . ? S1 Ag1 Ag2 52.18(7) 2_655 . ? S1 Ag1 Ag2 126.47(8) 3_665 . ? S1 Ag1 Ag2 100.78(7) . . ? S1 Ag1 Ag2 100.78(7) 2_655 2_655 ? S1 Ag1 Ag2 52.18(7) 3_665 2_655 ? S1 Ag1 Ag2 126.47(8) . 2_655 ? Ag2 Ag1 Ag2 76.10(4) . 2_655 ? S1 Ag1 Ag2 126.47(8) 2_655 3_665 ? S1 Ag1 Ag2 100.78(7) 3_665 3_665 ? S1 Ag1 Ag2 52.18(7) . 3_665 ? Ag2 Ag1 Ag2 76.10(4) . 3_665 ? Ag2 Ag1 Ag2 76.10(4) 2_655 3_665 ? P2 Ag2 S1 122.14(9) . 2_655 ? P2 Ag2 Cl1 111.35(11) . . ? S1 Ag2 Cl1 118.35(11) 2_655 . ? P2 Ag2 S2 105.42(10) . . ? S1 Ag2 S2 99.93(11) 2_655 . ? Cl1 Ag2 S2 92.87(7) . . ? P2 Ag2 Ag1 169.83(7) . . ? S1 Ag2 Ag1 49.41(7) 2_655 . ? Cl1 Ag2 Ag1 73.38(9) . . ? S2 Ag2 Ag1 82.92(7) . . ? Ag2 Cl1 Ag2 98.79(11) . 2_655 ? Ag2 Cl1 Ag2 98.79(11) . 3_665 ? Ag2 Cl1 Ag2 98.79(12) 2_655 3_665 ? P1 S1 Ag1 101.43(14) . . ? P1 S1 Ag2 97.05(14) . 3_665 ? Ag1 S1 Ag2 78.41(8) . 3_665 ? P1 S2 Ag2 113.42(16) . . ? O1 P1 O2 99.2(7) . . ? O1 P1 S2 111.2(4) . . ? O2 P1 S2 105.1(6) . . ? O1 P1 S1 110.7(5) . . ? O2 P1 S1 111.0(5) . . ? S2 P1 S1 117.95(18) . . ? C21 P2 C11 104.2(4) . . ? C21 P2 C5 104.5(5) . . ? C11 P2 C5 103.9(4) . . ? C21 P2 Ag2 114.0(3) . . ? C11 P2 Ag2 120.1(4) . . ? C5 P2 Ag2 108.7(3) . . ? C1 O1 P1 120.9(11) . . ? C3 O2 P1 129.0(15) . . ? C2 C1 O1 128(2) . . ? O2 C3 C4 115(2) . . ? C5 C5 P2 110.8(8) 10_657 . ? C16 C11 C12 119.2(11) . . ? C16 C11 P2 118.0(9) . . ? C12 C11 P2 122.8(8) . . ? C11 C12 C13 119.1(13) . . ? C14 C13 C12 120.3(15) . . ? C15 C14 C13 120.1(15) . . ? C14 C15 C16 120.4(15) . . ? C11 C16 C15 120.7(13) . . ? C22 C21 C26 117.2(10) . . ? C22 C21 P2 123.9(8) . . ? C26 C21 P2 118.9(8) . . ? C21 C22 C23 120.5(13) . . ? C24 C23 C22 122.0(15) . . ? C25 C24 C23 118.5(13) . . ? C24 C25 C26 120.0(13) . . ? C25 C26 C21 121.7(11) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.499 _refine_diff_density_min -0.794 _refine_diff_density_rms 0.089 #===END data_2b _database_code_depnum_ccdc_archive 'CCDC 254828' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H78 Ag4 Cl O6 P6 S6' _chemical_formula_weight 1704.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 19.8652(17) _cell_length_b 19.8652(17) _cell_length_c 33.169(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 11336(2) _cell_formula_units_Z 6 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 959 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 22.50 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5154 _exptl_absorpt_coefficient_mu 1.390 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6984 _exptl_absorpt_correction_T_max 0.9581 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10230 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4414 _reflns_number_gt 2417 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+290.5000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4414 _refine_ls_number_parameters 243 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1373 _refine_ls_R_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.1576 _refine_ls_wR_factor_gt 0.1297 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.6667 0.3333 0.07352(5) 0.0784(5) Uani 1 3 d S . . Ag2 Ag 0.58470(6) 0.19979(5) 0.00718(3) 0.0880(3) Uani 1 1 d . . . S1 S 0.79544(16) 0.33830(17) 0.08054(8) 0.0744(8) Uani 1 1 d . . . S2 S 0.70984(17) 0.18283(18) 0.01806(9) 0.0797(8) Uani 1 1 d . . . Cl1 Cl 0.6667 0.3333 -0.03063(15) 0.0799(14) Uani 1 3 d S . . P1 P 0.76071(17) 0.22533(17) 0.06992(8) 0.0699(8) Uani 1 1 d . . . P2 P 0.50240(16) 0.09378(15) -0.03765(7) 0.0604(7) Uani 1 1 d . . . O1 O 0.7056(5) 0.1733(5) 0.1048(2) 0.091(2) Uani 1 1 d . A . O2 O 0.8338(4) 0.2141(4) 0.0759(2) 0.082(2) Uani 1 1 d . . . C1 C 0.7239(8) 0.1869(8) 0.1465(4) 0.136(6) Uani 1 1 d D . . C2 C 0.730(2) 0.1162(14) 0.1606(10) 0.134(12) Uiso 0.50 1 d PD A 1 C2' C 0.6432(10) 0.153(2) 0.1662(9) 0.130(10) Uiso 0.50 1 d PD A 1 C3 C 0.6781(17) 0.2186(18) 0.1693(8) 0.117(9) Uiso 0.50 1 d PD A 2 C3' C 0.794(2) 0.226(4) 0.1751(16) 0.14(2) Uiso 0.25 1 d PD A 2 C3" C 0.681(4) 0.1020(14) 0.1614(19) 0.13(2) Uiso 0.25 1 d PD A 2 C4 C 0.8938(7) 0.2378(8) 0.0449(3) 0.085(3) Uani 1 1 d . . . H4A H 0.8820 0.2631 0.0228 0.102 Uiso 1 1 calc R . . C5 C 0.8926(9) 0.1680(10) 0.0294(5) 0.145(6) Uani 1 1 d . . . H5A H 0.8425 0.1334 0.0181 0.217 Uiso 1 1 calc R . . H5B H 0.9030 0.1423 0.0510 0.217 Uiso 1 1 calc R . . H5C H 0.9317 0.1826 0.0089 0.217 Uiso 1 1 calc R . . C6 C 0.9691(8) 0.2941(9) 0.0629(4) 0.136(6) Uani 1 1 d . . . H6A H 0.9666 0.3384 0.0725 0.204 Uiso 1 1 calc R . . H6B H 1.0092 0.3105 0.0429 0.204 Uiso 1 1 calc R . . H6C H 0.9805 0.2701 0.0849 0.204 Uiso 1 1 calc R . . C11 C 0.5516(6) 0.0866(7) -0.0830(3) 0.067(3) Uani 1 1 d . . . C12 C 0.5244(9) 0.0202(8) -0.1051(3) 0.113(5) Uani 1 1 d . . . H12A H 0.4800 -0.0250 -0.0970 0.136 Uiso 1 1 calc R . . C13 C 0.5629(12) 0.0204(11) -0.1396(4) 0.133(6) Uani 1 1 d . . . H13A H 0.5445 -0.0253 -0.1544 0.159 Uiso 1 1 calc R . . C14 C 0.6253(11) 0.0835(14) -0.1520(4) 0.129(7) Uani 1 1 d . . . H14A H 0.6502 0.0818 -0.1754 0.154 Uiso 1 1 calc R . . C15 C 0.6538(8) 0.1512(11) -0.1314(4) 0.118(5) Uani 1 1 d . . . H15A H 0.6972 0.1962 -0.1405 0.142 Uiso 1 1 calc R . . C16 C 0.6163(7) 0.1515(8) -0.0960(3) 0.097(4) Uani 1 1 d . . . H16A H 0.6359 0.1970 -0.0810 0.117 Uiso 1 1 calc R . . C21 C 0.4147(6) 0.0884(6) -0.0578(3) 0.066(3) Uani 1 1 d . . . C22 C 0.4154(8) 0.1555(7) -0.0666(3) 0.085(3) Uani 1 1 d . . . H22A H 0.4604 0.2028 -0.0619 0.102 Uiso 1 1 calc R . . C23 C 0.3509(10) 0.1556(10) -0.0822(4) 0.105(4) Uani 1 1 d . . . H23A H 0.3528 0.2022 -0.0884 0.126 Uiso 1 1 calc R . . C24 C 0.2854(9) 0.0874(12) -0.0882(4) 0.116(5) Uani 1 1 d . . . H24A H 0.2416 0.0872 -0.0983 0.139 Uiso 1 1 calc R . . C25 C 0.2819(9) 0.0193(10) -0.0799(4) 0.127(6) Uani 1 1 d . . . H25A H 0.2362 -0.0275 -0.0843 0.152 Uiso 1 1 calc R . . C26 C 0.3469(8) 0.0199(8) -0.0649(4) 0.101(4) Uani 1 1 d . . . H26A H 0.3448 -0.0270 -0.0594 0.121 Uiso 1 1 calc R . . C31 C 0.4676(6) 0.0014(6) -0.0110(3) 0.069(3) Uani 1 1 d . . . H31A H 0.4277 -0.0054 0.0082 0.083 Uiso 1 1 calc R . . H31B H 0.4443 -0.0410 -0.0302 0.083 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0765(7) 0.0765(7) 0.0823(10) 0.000 0.000 0.0382(3) Ag2 0.0916(7) 0.0775(7) 0.0816(6) -0.0166(5) -0.0045(5) 0.0325(6) S1 0.0713(19) 0.0746(19) 0.0733(17) -0.0003(14) -0.0074(14) 0.0334(16) S2 0.0700(19) 0.079(2) 0.0835(19) -0.0007(15) -0.0048(15) 0.0328(16) Cl1 0.0699(19) 0.0699(19) 0.100(4) 0.000 0.000 0.0350(10) P1 0.0715(19) 0.074(2) 0.0667(17) 0.0150(14) 0.0049(14) 0.0381(16) P2 0.0701(18) 0.0589(16) 0.0484(13) 0.0013(12) -0.0052(12) 0.0293(15) O1 0.100(6) 0.098(6) 0.075(5) 0.026(4) 0.017(4) 0.049(5) O2 0.085(5) 0.105(6) 0.071(5) 0.016(4) -0.001(4) 0.059(5) C1 0.157(15) 0.129(13) 0.083(10) 0.033(9) 0.001(9) 0.042(12) C4 0.077(9) 0.110(10) 0.082(8) 0.032(7) 0.017(7) 0.058(8) C5 0.158(16) 0.181(18) 0.143(13) 0.011(12) 0.033(11) 0.120(15) C6 0.083(10) 0.150(14) 0.150(13) 0.027(11) -0.016(9) 0.039(10) C11 0.076(8) 0.081(8) 0.049(6) 0.002(6) -0.008(5) 0.043(7) C12 0.166(14) 0.114(12) 0.058(7) -0.012(7) 0.002(8) 0.070(11) C13 0.20(2) 0.152(17) 0.079(10) -0.021(10) 0.004(11) 0.109(16) C14 0.142(16) 0.21(2) 0.060(9) 0.008(12) 0.014(10) 0.110(16) C15 0.090(10) 0.158(16) 0.085(10) 0.008(10) 0.009(8) 0.046(11) C16 0.090(10) 0.106(11) 0.072(8) 0.000(7) 0.006(7) 0.032(9) C21 0.075(8) 0.068(7) 0.049(6) 0.009(5) 0.007(5) 0.033(7) C22 0.112(10) 0.087(9) 0.071(7) 0.003(6) -0.001(7) 0.060(8) C23 0.131(13) 0.134(14) 0.096(9) 0.015(9) 0.007(10) 0.101(12) C24 0.090(12) 0.174(17) 0.101(10) 0.034(11) 0.002(9) 0.079(12) C25 0.093(11) 0.139(15) 0.127(12) 0.043(11) -0.014(9) 0.043(11) C26 0.089(10) 0.091(10) 0.114(10) 0.025(8) -0.022(8) 0.039(8) C31 0.068(7) 0.070(7) 0.057(6) 0.001(5) -0.012(5) 0.026(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 S1 2.521(3) . ? Ag1 S1 2.521(3) 3_665 ? Ag1 S1 2.521(3) 2_655 ? Ag1 Ag2 3.1955(14) . ? Ag1 Ag2 3.1955(14) 2_655 ? Ag1 Ag2 3.1955(14) 3_665 ? Ag2 P2 2.424(3) . ? Ag2 S1 2.588(3) 3_665 ? Ag2 Cl1 2.635(3) . ? Ag2 S2 2.695(3) . ? S1 P1 2.022(4) . ? S1 Ag2 2.588(3) 2_655 ? S2 P1 1.959(4) . ? Cl1 Ag2 2.635(3) 2_655 ? Cl1 Ag2 2.635(3) 3_665 ? P1 O1 1.572(7) . ? P1 O2 1.589(7) . ? P2 C21 1.818(11) . ? P2 C31 1.832(10) . ? P2 C11 1.837(10) . ? O1 C1 1.423(14) . ? O2 C4 1.462(12) . ? C1 C3 1.5398(10) . ? C1 C3' 1.5399(11) . ? C1 C2' 1.5400(10) . ? C1 C3" 1.5401(10) . ? C1 C2 1.5401(10) . ? C4 C5 1.469(17) . ? C4 C6 1.472(16) . ? C11 C16 1.357(14) . ? C11 C12 1.363(15) . ? C12 C13 1.374(18) . ? C13 C14 1.31(2) . ? C14 C15 1.36(2) . ? C15 C16 1.390(17) . ? C21 C22 1.360(14) . ? C21 C26 1.373(15) . ? C22 C23 1.383(16) . ? C23 C24 1.343(18) . ? C24 C25 1.348(19) . ? C25 C26 1.379(17) . ? C31 C31 1.506(18) 10_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ag1 S1 119.16(2) . 3_665 ? S1 Ag1 S1 119.16(2) . 2_655 ? S1 Ag1 S1 119.16(2) 3_665 2_655 ? S1 Ag1 Ag2 100.48(7) . . ? S1 Ag1 Ag2 52.23(7) 3_665 . ? S1 Ag1 Ag2 128.41(8) 2_655 . ? S1 Ag1 Ag2 52.23(7) . 2_655 ? S1 Ag1 Ag2 128.41(8) 3_665 2_655 ? S1 Ag1 Ag2 100.48(7) 2_655 2_655 ? Ag2 Ag1 Ag2 77.80(4) . 2_655 ? S1 Ag1 Ag2 128.41(8) . 3_665 ? S1 Ag1 Ag2 100.48(7) 3_665 3_665 ? S1 Ag1 Ag2 52.23(7) 2_655 3_665 ? Ag2 Ag1 Ag2 77.80(4) . 3_665 ? Ag2 Ag1 Ag2 77.80(4) 2_655 3_665 ? P2 Ag2 S1 121.27(10) . 3_665 ? P2 Ag2 Cl1 113.05(12) . . ? S1 Ag2 Cl1 117.31(11) 3_665 . ? P2 Ag2 S2 103.72(10) . . ? S1 Ag2 S2 102.23(10) 3_665 . ? Cl1 Ag2 S2 92.60(7) . . ? P2 Ag2 Ag1 170.41(8) . . ? S1 Ag2 Ag1 50.35(7) 3_665 . ? Cl1 Ag2 Ag1 71.95(10) . . ? S2 Ag2 Ag1 83.83(7) . . ? P1 S1 Ag1 99.44(14) . . ? P1 S1 Ag2 99.46(13) . 2_655 ? Ag1 S1 Ag2 77.42(9) . 2_655 ? P1 S2 Ag2 111.89(16) . . ? Ag2 Cl1 Ag2 99.21(13) 2_655 . ? Ag2 Cl1 Ag2 99.21(13) 2_655 3_665 ? Ag2 Cl1 Ag2 99.21(13) . 3_665 ? O1 P1 O2 101.6(4) . . ? O1 P1 S2 108.8(3) . . ? O2 P1 S2 111.1(3) . . ? O1 P1 S1 109.9(3) . . ? O2 P1 S1 107.8(3) . . ? S2 P1 S1 116.59(18) . . ? C21 P2 C31 104.3(5) . . ? C21 P2 C11 103.0(4) . . ? C31 P2 C11 105.4(5) . . ? C21 P2 Ag2 119.2(4) . . ? C31 P2 Ag2 109.1(3) . . ? C11 P2 Ag2 114.6(4) . . ? C1 O1 P1 124.2(8) . . ? C4 O2 P1 121.4(6) . . ? O1 C1 C3 114.0(15) . . ? O1 C1 C3' 141(3) . . ? C3 C1 C3' 93(3) . . ? O1 C1 C2' 102.6(15) . . ? C3 C1 C2' 43.4(15) . . ? C3' C1 C2' 116(3) . . ? O1 C1 C3" 99(3) . . ? C3 C1 C3" 100(3) . . ? C3' C1 C3" 103(4) . . ? C2' C1 C3" 60(3) . . ? O1 C1 C2 104.6(16) . . ? C3 C1 C2 124(2) . . ? C3' C1 C2 79(3) . . ? C2' C1 C2 90.6(19) . . ? C3" C1 C2 33(3) . . ? O2 C4 C5 108.4(11) . . ? O2 C4 C6 108.4(11) . . ? C5 C4 C6 113.0(12) . . ? C16 C11 C12 118.4(11) . . ? C16 C11 P2 118.3(9) . . ? C12 C11 P2 123.2(10) . . ? C11 C12 C13 119.6(15) . . ? C14 C13 C12 121.5(17) . . ? C13 C14 C15 121.0(16) . . ? C14 C15 C16 118.1(15) . . ? C11 C16 C15 121.4(13) . . ? C22 C21 C26 117.3(11) . . ? C22 C21 P2 118.8(9) . . ? C26 C21 P2 123.9(9) . . ? C21 C22 C23 121.8(13) . . ? C24 C23 C22 119.0(14) . . ? C23 C24 C25 121.3(15) . . ? C24 C25 C26 119.1(15) . . ? C21 C26 C25 121.4(13) . . ? C31 C31 P2 111.7(9) 10_655 . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.188 _refine_diff_density_min -0.696 _refine_diff_density_rms 0.101